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Yerekana karuseli ya sisitemu eshatu icyarimwe. Koresha Utubuto na Ibikurikira kugirango unyuze mumashusho atatu icyarimwe, cyangwa ukoreshe utubuto twa slide kumpera kugirango wimuke unyuze mubice bitatu icyarimwe.
Ibyuma bikoreshwa cyane bitagira umuyonga hamwe nuburyo bwakorewe birwanya kwangirika mubihe bidukikije bitewe na passivation igizwe na oxyde ya chromium. Kwangirika no gutwarwa nicyuma mubisanzwe bifitanye isano no kurimbuka kwizi nzego, ariko gake cyane no kugaragara nkuburinganire bwimiterere, bitewe nurwego rwa microscopique. Muri iki gikorwa, imiterere ya nanoscale yubutaka butandukanye, igaragazwa na microscopi ya spekitroscopique hamwe nisesengura rya chemometrike, mu buryo butunguranye byiganjemo kuvunika no kwangirika kwa cerium ikonje yahinduwe na super duplex idafite ibyuma 2507 (SDSS) mugihe cyo guhindura ubushyuhe bwayo. Nubwo microscopi ya X-ray yerekanaga uburyo bumwe busa nuburinganire bwa Cr2O3, imikorere ya passivation ya SDSS ikonje ikonje yari ikennye kubera ikwirakwizwa ryaho rya nanoisland ya Fe3 + ikungahaye kuri Fe / Cr oxyde. Ubu bumenyi bwa atome butanga ubumenyi bwimbitse bwo kwangirika kwicyuma kandi biteganijwe ko buzafasha kurwanya ruswa yibyuma bisa cyane.
Kuva havumburwa ibyuma bitagira umwanda, imiti irwanya ruswa ya ferrochrome yitiriwe chromium, ikora oxyde ikomeye / oxyhydroxide kandi ikagaragaza imyitwarire ishimishije mubidukikije. Ugereranije nicyuma gisanzwe (austenitis na ferritic) ibyuma 1, 2, 3, super duplex ibyuma bitagira umuyonga (SDSS) bifite imbaraga zo kurwanya ruswa hamwe nibikoresho byiza bya mashini. Kongera imbaraga za mashini zituma ibishushanyo byoroheje kandi byoroshye. Ibinyuranye na byo, ubukungu bwa SDSS bufite imbaraga nyinshi zo kurwanya ruswa no gutoboka, bigatuma ubuzima bumara igihe kirekire, bityo bikagura uburyo bwo kurwanya umwanda, ibikoresho by’imiti, n’inganda zikomoka kuri peteroli na gaze mu mahanga4. Nyamara, intera ntoya yubushyuhe bwo kuvura ubushyuhe hamwe nubushobozi buke bubangamira ishyirwa mubikorwa ryabyo. Kubwibyo, SDSS yahinduwe kugirango itezimbere imikorere yavuzwe haruguru. Kurugero, guhindura Ce byatangijwe muri SDSS 2507 (Ce-2507) hamwe na azote nyinshi 6,7,8. Ikintu kidasanzwe cy'ubutaka (Ce) ku gipimo gikwiye cya 0.08 wt.% Kigira ingaruka nziza kumiterere ya DSS, kubera ko itunganya neza ingano nimbaraga zimbibi. Kwambara no kwangirika, imbaraga zingana nimbaraga zitanga umusaruro, hamwe nubushyuhe bwo gukora nabyo biratera imbere9. Umubare munini wa azote urashobora gusimbuza nikel ihenze, bigatuma SDSS ihenze cyane10.
Vuba aha, SDSS yahinduwe muburyo bwubushyuhe butandukanye (cryogenic, imbeho nubushyuhe) kugirango igere kumikorere myiza ya mashini 6.7,8. Nyamara, uburyo bwiza bwo kurwanya ruswa ya SDSS bitewe no kuba hari firime yoroheje ya okiside hejuru yibasiwe nibintu byinshi nko kuvuka kwa heterogeneité bitewe nuko hariho ibyiciro bitandukanye bitandukanya imbibi zinyuranye, imvura idashaka hamwe nigisubizo gitandukanye. deformations zicyiciro cya austenitis na ferritic7. Kubwibyo, ubushakashatsi bwimiterere ya microscopique yumutungo wamafilime kugeza kurwego rwuburyo bwa elegitoronike biba ingenzi mugusobanukirwa kwangirika kwa SDSS kandi bisaba tekinike yubushakashatsi. Kugeza ubu, uburyo bwibanda ku buso nka Auger electron spectroscopy11 na X-ray fotoelectron spectroscopy12,13,14,15 hamwe na microscopi ya X-ray ifotora (HAX-PEEM) 16 muri rusange ntibyashoboye kumenya itandukaniro ryimiti mubice byubutaka. imiterere yimiti yibintu bimwe ahantu hatandukanye kumwanya wa nanoscale. Ubushakashatsi bwinshi buherutse gukorwa bufitanye isano na okiside ya chromium hamwe n’imyitwarire igaragara yo kwangirika kwicyuma cya austenitis cyuma 17, ibyuma bya martensitike 18 na SDSS19,20. Nyamara, ubu bushakashatsi bwibanze ahanini ku ngaruka za Cr heterogeneité (urugero, Cr3 + okiside ya leta) ku kurwanya ruswa. Gutandukana kuruhande muri okiside yibintu bishobora guterwa nibintu bitandukanye bifite ibice bimwe, nka okiside ya fer. Izi mvange, zarazwe ingano ntoya bitewe nubuvuzi bwa termo-mashini, ziri hafi yizindi, ariko ziratandukanye mubigize hamwe na okiside leta 16,21. Kubwibyo, kugirango hamenyekane ibice bya firime ya okiside hamwe nibishobora gukurikiraho, birakenewe gusobanukirwa ubutumburuke bwurwego rwa microscopique. Nubwo ibi bisabwa, igereranya ryinshi nka heterogeneité kuruhande rwa okiside, cyane cyane kuri Fe kurwego rwa nano- na atome, iracyabura, kandi ihuriro ryayo hamwe no kurwanya ruswa iracyashakishwa. Kugeza vuba aha, imiterere yimiti yibintu bitandukanye, nka Fe na Ca22, ku byitegererezo by'ibyuma yaranzwe mu buryo bworoshye hakoreshejwe microscopi ya X-ray yoroheje ya elegitoronike (X-PEEM) mu bikoresho by'imirasire ya nanoscale synchrotron. X-PEEM ifatanije na X-ray ikurura imiti ya X-ray (XAS), X-PEEM ituma ibipimo bya XAS bifite imiterere ihanitse kandi igaragara, itanga amakuru yimiti yerekeranye nibintu bigize imiterere yimiterere yabyo hamwe nuburinganire bwimiterere yabantu kugeza kuri nanometero makumyabiri na eshatu. . Uku kwitegereza spekitromicroscopique yibitangira byorohereza kwitegereza imiti kandi birashobora kwerekana impinduka zimiti mumwanya wicyuma kitigeze gikorerwa iperereza.
Ubu bushakashatsi bwaguye ibyiza bya PEEM mugutahura itandukaniro ryimiti kuri nanoscale kandi ryerekana uburyo bwimbitse bwa atome-urwego rwo gusesengura uburyo bwo gusobanukirwa imyitwarire ya ruswa ya Ce-2507. Ikoresha uburyo bwa K-busobanura 24 bwa chimometrike kugirango ushushanye ikarita yisi yose (hetero) ubutinganyi bwibintu birimo, ibihugu byimiti bigaragazwa mubarurishamibare. Bitandukanye no kwangirika kwatangijwe no gusenya firime ya chromium oxyde mu bihe gakondo, passivasi nkeya hamwe no kurwanya ruswa yo hasi kuri ubu biterwa na nanoisland ikungahaye kuri Fe3 + hafi ya Fe / Cr oxyde, ishobora kuba ibintu birinda umutekano. Okiside isenya firime yerekana akadomo kandi igatera ruswa.
Imyitwarire ibora ya SDSS 2507 yahinduwe yasuzumwe bwa mbere hakoreshejwe ibipimo by'amashanyarazi. Ku mutini. Igishushanyo 1 kirerekana umurongo wa Nyquist na Bode kuburugero rwatoranijwe muri acide (pH = 1) igisubizo cyamazi ya FeCl3 mubushyuhe bwicyumba. Byahiswemo electrolyte ikora nka agent ikomeye ya okiside, iranga impengamiro ya firime ya passivation yo gucika. Nubwo ibikoresho bitigeze bihinduka neza mubushyuhe bwicyumba, isesengura ryatanze ubushishozi kubintu bishobora kunanirwa no kwangirika nyuma. Umuzunguruko uhwanye (Igishusho 1d) wakoreshejwe kugirango uhuze amashanyarazi ya electrochemical impedance spectroscopy (EIS), kandi ibisubizo bihuye bikwiranye nimbonerahamwe ya 1 Muri EIS spectroscopy, radiyo yumuzingi irashobora gufatwa nkurwanya polarisiyasi (Rp) 25,26. Rp yumuti wavuwe mumurongo wa 1 ni nka 135 kΩ cm - 2, nyamara, indangagaciro zumuhanda ushyushye kandi ukonje ukonje cyane ni hasi cyane, 34.7 na 2,1 kΩ cm - 2. Iri gabanuka rikomeye muri Rp ryerekana ingaruka mbi zo guhindura plastike kuri passivation no kurwanya ruswa, nkuko bigaragara muri raporo zabanjirije 27,28,29,30.
a Nyquist, b, c Bode impedance nigishushanyo cyicyiciro, hamwe na d ihwanye nicyitegererezo cyumuzunguruko, aho RS irwanya electrolyte, Rp niyo irwanya polarisiyasi, naho QCPE ni oxyde yibintu bihoraho bikoreshwa mugushushanya ubushobozi butari bwiza (n). Ibipimo bya EIS bikozwe kubishobora kuzunguruka.
Icyarimwe icyarimwe cyerekanwe mugace ka Bode, hamwe na plateau mumurongo mwinshi ugereranya electrolyte irwanya RS26. Mugihe inshuro zigabanuka, impedance iriyongera kandi inguni itari nziza iboneka, byerekana ubushobozi bwiganje. Inguni yicyiciro iriyongera, igumana ntarengwa hejuru yumurongo mugari ugereranije, hanyuma igabanuka (Ishusho 1c). Nyamara, muri ibyo bihe uko ari bitatu, iyi ntarengwa iracyari munsi ya 90 °, byerekana imyitwarire idahwitse ya capacitif kubera gutatanya ubushobozi. Rero, QCPE icyiciro cya buri gihe (CPE) ikoreshwa muguhagararira ubushobozi bwimikoreshereze yimikorere ituruka kumurongo wo hejuru cyangwa kutagira ubumuntu, cyane cyane kurwego rwa atome, geometrike ya fractale, porotoro ya electrode, ubushobozi butari bumwe, na geometrie ifite ishusho ya electrode 31,32. CPE inzitizi:
aho j numubare wibitekerezo kandi ω ni inshuro zingana. QCPE numuyoboro wigenga uhoraho ugereranije nu gice gifunguye cya electrolyte. n numubare wububasha butagira urugero usobanura gutandukana kwa capacitori kuva capacitance nziza, nukuvuga ko hafi ya n ari 1, uko CPE yegereye ubushobozi gusa, mugihe niba n yegereye zeru, bigaragara ko irwanya. Gutandukana kwa n, hafi ya 1, byerekana imyitwarire idahwitse ya capacitif yubuso nyuma yikizamini cya polarisiyasi. QCPE yubukonje bwa SDSS irarenze cyane ugereranije na bagenzi bayo, bivuze ko ubwiza bwubuso butari bumwe.
Bikwiranye nibintu byinshi birwanya kwangirika kwibyuma bitagira umwanda, ugereranije nibiri hejuru ya Cr yibiri muri SDSS mubisanzwe bivamo kurwanya ruswa cyane ya SDSS bitewe nuko hari firime ya okiside irinda umubiri hejuru17. Amafirime nkaya asanzwe akungahaye kuri Cr3 + oxyde na / cyangwa hydroxide, cyane cyane hamwe na Fe2 +, Fe3 + oxyde na / cyangwa (oxy) hydroxide33. Nuburyo bumwe buringaniye, passivasi ya oxyde, kandi ntagaragara hejuru yubutaka ukurikije ibipimo bya microscopique6,7, imyitwarire yo kwangirika ya SDSS ishyushye kandi ikonje ikonje iratandukanye, kubwibyo ubushakashatsi bwimbitse buranga microstructural burakenewe kugirango hahindurwe ibyuma.
Microstructure yibyuma bidafite ibyuma byahinduwe byizwe muburyo bwinshi hakoreshejwe imirasire ya synchrotron ifite ingufu nyinshi X-imirasire (Ishusho yinyongera 1, 2). Isesengura rirambuye ritangwa mu makuru yinyongera. Nubwo hari ubwumvikane rusange kubwoko bwicyiciro cyingenzi, habonetse itandukaniro mubice byinshi byiciro byabonetse, biri kurutonde rwinyongera ya 1.Ibinyuranyo bishobora guterwa nuduce duto twa fonomogeneous hejuru no mubunini, ibyo bikaba biterwa nuburebure butandukanye bwa X-ray (XRD). ) hamwe nimbaraga zitandukanye zamafoto yibyabaye34. Ugereranije uduce duto twa austenite mubice bikonje byagenwe na XRD biva muri laboratoire byerekana passivasi nziza hanyuma irwanya ruswa neza35, mugihe ibisubizo nyabyo kandi bibarurishamibare byerekana inzira zinyuranye mubice by'ibice. Byongeye kandi, kurwanya ruswa kwangirika kandi biterwa nurwego rwo gutunganya ingano, kugabanuka kw ingano, kwiyongera kwa microdeformations hamwe nubucucike bwa dislokisiyo bibaho mugihe cyo kuvura imiti 36,37,38. Ingero zakozwe zishyushye zerekanaga imiterere yimbuto nyinshi, yerekana ingano nini ya micron, mugihe impeta yoroshye yagaragaye mubigero bikonje bikonje (Ishusho yinyongera 3) byerekanaga kunonosora ingano kuri nanosize mubikorwa byabanjirije. Ibi bigomba gutonesha firime. gushiraho no kongera imbaraga zo kurwanya ruswa. Ubucucike buri hejuru busanzwe bujyanye no kurwanya umwobo wo hasi, ibyo bikaba bihuza neza nu gupima amashanyarazi.
Impinduka mumiterere ya chimique ya microdomaine yibintu byingenzi byizwe kuri gahunda hakoreshejwe X-PEEM. Nubwo hari ibintu byinshi bivangavanze, Cr, Fe, Ni na Ce39 byatoranijwe hano, kubera ko Cr aricyo kintu cyingenzi cyo gukora firime ya pasiporo, Fe nikintu nyamukuru cyibyuma, kandi Ni yongerera passiyo kandi ikaringaniza icyiciro cya ferrite-austenitis. Imiterere no guhindura niyo ntego ya Ce. Muguhuza ingufu za synchrotron beam, XAS yafashe ibintu nyamukuru biranga Cr (L2.3 edge), Fe (L2.3 edge), Ni (L2.3 edge), na Ce (M4.5 edge) uhereye hejuru. -2507 SDSS. Isesengura ryamakuru ryakozwe ryakozwe mugushyiramo ingufu za kalibrasi hamwe namakuru yatangajwe (urugero: XAS kuri Fe L2, imbavu 40,41).
Ku mutini. Igishushanyo cya 2 cyerekana X-PEEM amashusho yubushyuhe bukora (Igishusho 2a) hamwe no gukonjesha (Ishusho 2d) Ce-2507 SDSS hamwe na XAS Cr na Fe L2,3 bihuye kumyanya yihariye. Uruhande rwa L2,3 XAS rugaragaza leta ya 3d idakoreshwa na electron nyuma yo gufotora kuri 2p3 / 2 (L3 edge) na 2p1 / 2 (L2 edge) kuzenguruka-kuzenguruka. Amakuru ajyanye na valence leta ya Cr yabonetse mubisesengura rya X-ray yo gusesengura impande ya L2,3 kumashusho 2b, d. Kugereranya. 42, 43 yerekanye ko impinga enye A (578.3 eV), B (579.5 eV), C (580.4 eV), na D (582.2 eV) zagaragaye hafi yinkombe ya L3, zigaragaza octahedral Cr3 + ion, ihuye na Cr2O3. Ubushakashatsi bwakorewe ubushakashatsi burahuza nibiharuro, nkuko bigaragara mu kibaho b na e, byabonetse mu mibare myinshi ya kirisiti yo kubara kuri interineti ya Cr L2.3 ukoresheje umurima wa kirisiti ya 2.0 eV44. Ubuso bwombi bwa SDSS bushyushye kandi bukonje bukonje hamwe na layer ya Cr2O3.
ishusho yubushyuhe ya X-PEEM ishyushye-SDSS ihuye nuruhande b Cr L2.3 nuruhande c Fe L2.3, d Ishusho yubushyuhe X-PEEM ya SDSS ikonje ikonje ihuye na e Cr L2.3 na f Fe L2.3 kuruhande (e). Ikirangantego cya XAS cyateguwe ahantu hatandukanye hagaragara ku mashusho yubushyuhe (a, d) n'umurongo utudomo twa orange muri (b) na (e) ugereranya XAS yerekanwe ya Cr3 + ifite agaciro kangana na 2.0 eV. Ku mashusho ya X-PEEM, palette yumuriro ikoreshwa mugutezimbere amashusho asomeka, aho amabara kuva mubururu kugeza kumutuku aringaniye nuburemere bwokwinjira kwa X-ray (kuva hasi kugeza hejuru).
Hatitawe ku bidukikije byimiti yibintu byuma, imiterere yimiti yongeweho ya Ni na Ce ivanga ibintu byombi byombi byakomeje kuba bimwe. Igishushanyo cy'inyongera. Ku mutini. 5-9 herekana amashusho X-PEEM hamwe na XAS yerekanwe kuri Ni na Ce kumwanya utandukanye hejuru yubushyuhe bukora kandi bukonje. Ni XAS yerekana okiside ya Ni2 + hejuru yubuso bwose bwapimwe bwubushyuhe bukora kandi bukonje (Ikiganiro cyinyongera). Birashimishije ko mugihe cyibishushanyo bishyushye byakozwe, ikimenyetso cya XAS cya Ce ntikigaragara, mugihe spekiteri ya Ce3 + yikigereranyo gikonje igaragara mugihe kimwe. Kwihweza ibibanza bya Ce mubitegererezo bikonje byerekanaga ko Ce ibaho muburyo bwimvura.
Muri SDSS yahinduwe neza, nta mpinduka zubatswe zaho muri XAS zagaragaye ku nkombe ya Fe L2.3 (Ishusho 2c). Ariko, nkuko bigaragara ku gishushanyo. 2f, Fe matrix ya microscopique ihindura imiterere yimiti kubintu birindwi byatoranijwe muburyo bukonje bwa SDSS. Byongeye kandi, kugirango tubone igitekerezo nyacyo cyimpinduka zabaye muri leta ya Fe ahantu hatoranijwe ku gishushanyo cya 2f, hakozwe ubushakashatsi bw’ubutaka bwaho (Ishusho ya 3 n’inyongera ya 10) aho hatoranijwe uturere duto tuzengurutse. XAS yerekanwe ya Fe L2,3 ya sisitemu ya α-Fe2O3 na okiside ya Fe2 + octahedral yagereranijwe ikoresheje imibare myinshi ya kirisiti yo kubara ikoresheje imirima ya kristu ya 1.0 (Fe2 +) na 1.0 (Fe3 +) 44. Twibutse ko α-Fe2O3 na γ-Fe2O3 bifite ibipimo bitandukanye byaho 45,46, Fe3O4 ifite ibice byombi bya Fe2 + & Fe3 +, 47, na FeO45 nkibisanzwe bihuza Fe2 + oxyde (3d6). Twibutse ko α-Fe2O3 na γ-Fe2O3 bifite ibice bitandukanye byaho 45,46, Fe3O4 ifite ihuriro ryombi rya Fe2 + & Fe3 +, 47, na FeO45 nkibisanzwe bihuza Fe2 + oxyde (3d6).Menya ko α-Fe2O3 na γ-Fe2O3 bifite ibice bitandukanye byaho 45,46, Fe3O4 ikomatanya Fe2 + na Fe3 +, 47 na FeO45 muburyo bwa oxyde ihwanye na Fe2 + (3d6).Menya ko α-Fe2O3 na γ-Fe2O3 bifite ibice bitandukanye byaho 45,46, Fe3O4 ifite guhuza Fe2 + na Fe3 +, 47 na FeO45 ikora nkibisanzwe byemewe na Fe2 + oxyde (3d6). Fe3 + ion zose muri α-Fe2O3 zifite gusa Oh imyanya, mugihe γ-Fe2O3 ubusanzwe igaragazwa nka Fe3 + t2g [Fe3 + 5 / 3V1 / 3] urugero O4 spinel ifite imyanya mungero imyanya. Kubwibyo, Fe3 + ion muri γ-Fe2O3 zifite imyanya yombi Td na Oh. Nkuko byavuzwe mubikorwa byabanjirije iki, nubwo igipimo cyimbaraga zombi ziratandukanye, igipimo cyimbaraga zabo eg / t2g ni ≈1, mugihe muriki gihe igipimo cyimbaraga zagaragaye urugero / t2g ni nka 1. Ibi birabuza ko Fe3 + yonyine ishobora kuba muri uru rubanza. Urebye ikibazo cya Fe3O4 hamwe na Fe2 + na Fe3 +, birazwi ko ikintu cya mbere kidakomeye (gikomeye) mugice cya L3 cya Fe cyerekana ikintu gito (kinini) kidahwitse muri leta ya t2g. Ibi bireba Fe2 + (Fe3 +), byerekana kwiyongera mubimenyetso byambere byerekana ubwiyongere bwibiri muri Fe2 + 47. Ibisubizo byerekana ko Fe2 + na γ-Fe2O3, α-Fe2O3 na / cyangwa Fe3O4 byiganje hejuru yubukonje buzengurutse ibice.
Kwagura amafoto yagutse ya elegitoroniki amashusho yubushyuhe bwa (a, c) na (b, d) XAS yerekanwe kuruhande rwa Fe L2,3 kumyanya itandukanye ahantu hatandukanye mu turere twatoranijwe 2 na E mubishushanyo. 2d.
Amakuru yubushakashatsi yabonetse (Igicapo 4a hamwe ninyongera 11) yateguwe kandi ugereranije nayandi masoko meza 40, 41, 48. Ahanini, ubwoko butatu butandukanye bwakorewe ubushakashatsi bwa Fe L-edge XAS (XAS-1, XAS-2 na XAS-3: Ishusho 4a) bwagaragaye ahantu hatandukanye. By'umwihariko, icyerekezo gisa na 2-a (cyiswe XAS-1) ku gishushanyo cya 3b cyagaragaye mu karere kose gashimishije, hagakurikiraho icyerekezo cya 2-b (cyanditseho XAS-2), naho icyerekezo gisa na E-3 cyagaragaye mu mbuto. 3d (byitwa XAS-3) byagaragaye ahantu runaka. Mubisanzwe, ibipimo bine bikoreshwa mukumenya imiterere ya valence igaragara murugero rwiperereza: (1) L3 na L2 ibiranga ibintu, (2) imyanya yingufu za L3 na L2, (3) itandukaniro ryingufu za L3-L2, (4) L2 ubukana bwa L2 / L3. Ukurikije uko bigaragara (Ishusho 4a), ibice bitatu byose bigize Fe, aribyo Fe0, Fe2 +, na Fe3 +, biboneka hejuru ya SDSS yize. Ikigereranyo cyimbaraga zabazwe L2 / L3 nazo zerekanaga ko hariho ibice bitatu byose.
a Indorerezi eshatu zitandukanye zigeragezwa (imirongo ihamye XAS-1, XAS-2 na XAS-3 ihuye na 2-a, 2-b na E-3 ku gishushanyo cya 2 no ku gishushanyo cya 3) ugereranije na XAS igereranya igereranya, octahedrons Fe2 +, Fe3 +, indangagaciro zo mu murima zingana na 1.0 eV na 1.5 eV, bikurikiranye X-XAS .
Gukomatanya umurongo (LCF) bihuye n'ibipimo bitatu40.41,48 byakoreshejwe mukugereranya ibice bya oxyde de fer. LCF yashyizwe mubikorwa bitatu byatoranijwe Fe L-edge XAS yerekana itandukaniro ryinshi, aribyo XAS-1, XAS-2 na XAS-3, nkuko bigaragara ku gishushanyo cya 4b - d. Kubikoresho bya LCF, 10% Fe0 byasuzumwe muburyo bwose bitewe numutwe muto twabonye mumibare yose no kuba ibyuma bya fer ari byo bigize ibyuma. Mubyukuri, ubujyakuzimu bwa X-PEEM kuri Fe (~ 6 nm) 49 nini kuruta ubunini bwagereranijwe bwa oxydeire (gato> 4 nm), butuma hamenyekana ibimenyetso biva muri materique y'icyuma (Fe0) munsi ya passivation. Mubyukuri, ubujyakuzimu bwa X-PEEM kuri Fe (~ 6 nm) 49 nini kuruta ubunini bwagereranijwe bwa oxydeire (gato> 4 nm), butuma hamenyekana ibimenyetso biva muri materique y'icyuma (Fe0) munsi ya passivation. Действительно, Кнаная глубина X-PEEM для Fe (~ 6 нм) 49 больше, чем предполагаемая толщина слоя окисления (немного> 4 нм), что позволяет обнаружить у от железной матрицы (Fe0) Mubyukuri, probe X-PEEM ubujyakuzimu bwa Fe (~ 6 nm) 49 iruta ubwinshi bwafashwe nkuburinganire bwurwego rwa okiside (gato> 4 nm), bigatuma bishoboka kumenya ibimenyetso biva muri materique yicyuma (Fe0) munsi ya passivation.Mubyukuri, X-PEEM itahura Fe (~ 6 nm) 49 yimbitse kuruta uburebure buteganijwe bwurwego rwa oxyde (hejuru ya 4 nm), bigatuma habaho ibimenyetso biva muri materique yicyuma (Fe0) munsi ya passivation. Ihuriro ritandukanye rya Fe2 + na Fe3 + ryakozwe kugirango haboneke igisubizo cyiza gishoboka kumibare yubushakashatsi yagaragaye. Ku mutini. Igicapo 4b cerekana guhuza Fe2 + na Fe3 + murwego rwa XAS-1, aho ibipimo bya Fe2 + na Fe3 + byegeranye, hafi 45%, byerekana imiterere ya okiside ivanze ya Fe. Mugihe kuri XAS-2 igaragara, ijanisha rya Fe2 + na Fe3 + rihinduka ~ 30% na 60%. Ibiri muri Fe2 + biri munsi yibya Fe3 +. Ikigereranyo cya Fe2 + na Fe3 cya 1: 2 bivuze ko Fe3O4 ishobora gukorwa ku kigereranyo kimwe cya Fe ion. Mubyongeyeho, kuri XAS-3 ya ecran, ijanisha rya Fe2 + na Fe3 + ryahindutse ~ 10% na 80%, byerekana ihinduka ryinshi rya Fe2 + kuri Fe3 +. Nkuko byavuzwe haruguru, Fe3 + irashobora kuva kuri α-Fe2O3, γ-Fe2O3 cyangwa Fe3O4. Kugirango usobanukirwe ninkomoko ya Fe3 +, XAS-3 yerekanwe hamwe hamwe nibipimo bitandukanye bya Fe3 + mubishusho 4e byerekana guhuza nibipimo byombi iyo Peak B isuzumwe. Nyamara, ubukana bwigitugu (A: kuva kuri Fe2 +) hamwe nuburinganire bwimbaraga B / A byerekana ko urwego rwa XAS-3 rwegereye ariko ntirumeze nka γ-Fe2O3. Ugereranije ninshi γ-Fe2O3, ubukana bwa Fe 2p XAS bwimpinga ya SDSS buri hejuru cyane (Ishusho 4e), byerekana ubukana bwa Fe2 +. Nubwo ibice bya XAS-3 bisa nkibya γ-Fe2O3, aho Fe3 + igaragara haba mumyanya yombi ya Oh na Td, kumenyekanisha imiterere ya valence zitandukanye no guhuza gusa na L2,3 cyangwa igipimo cya L2 / L3 kiracyari ikibazo. ingingo isubirwamo kenshi kubera ubunini bwibintu bitandukanye bigira uruhare rwanyuma41.
Usibye ivangura rishingiye ku miterere y’imiterere y’uturere twatoranijwe dushimishijwe haruguru, isuzumabumenyi ry’imiti ku isi y’ibintu by'ingenzi Cr na Fe ryasuzumwe no gushyira mu byiciro XAS yerekanwe ku cyitegererezo hakoreshejwe uburyo bwa K-buryo bwo guhuriza hamwe. Umwirondoro wuruhande Cr L washyizweho muburyo bwo gukora ibice bibiri byiza byakwirakwijwe ahantu hatanzwe kandi hashyushye bikonje byerekanwe mubishushanyo. 5. Biragaragara ko nta mpinduka zubatswe zaho zagaragaye, kubera ko centroide ebyiri za XAS Cr zisa cyane. Iyi shusho yerekana ibice bibiri bisa nkaho bihuye na Cr2O342, bivuze ko ibice bya Cr2O3 bigabanijwe kimwe kuri SDSS.
ihuriro rya K-risobanura L-edge Cr uturere, b bihuye na XAS centroide. Ibisubizo bya K-bisobanura X-PEEM kugereranya SDSS ikonje: c ihuriro rya K-bisobanura uturere twa Cr L2,3 na d bihuye na XAS centroide.
Kugirango ugaragaze ikarita igoye cyane ya FeL, ikarita enye na eshanu zashyizwe hamwe hamwe na centroide zifitanye isano (kugabana ibintu) zikoreshwa muburyo bushyushye kandi bukonje bukonje. Kubwibyo, ijanisha (%) rya Fe2 + na Fe3 + rirashobora kuboneka muguhindura LCF yerekanwe kumashusho.4. Pseudoelectrode ishobora kuba Epseudo nkigikorwa cya Fe0 yakoreshejwe muguhishurira mikorobe ya inhomogeneitike ya firime ya oxyde yo hejuru. Epseudo igereranijwe hafi namategeko yo kuvanga,
aho \ (\ rm {E} _ {\ rm {Fe} / \ rm {Fe} ^ {2 + (3 +)}} \) bingana \ (\ rm {Fe} + 2e ^ - \ kugeza \ rm {Fe} ^ {2 + (3 +)} \), ni 0.440 na 0.036 V. Uturere dufite ubushobozi buke bufite ibintu byinshi byo murwego rwa Fe3 +. Ikwirakwizwa rishobora gukwirakwizwa mubushuhe bwahinduwe bifite imiterere itandukanye hamwe nimpinduka ntarengwa ya 0.119 V (Ishusho 6a, b). Uku gukwirakwiza gushobora kuba gufitanye isano rya bugufi n'ubutaka (Ishusho 6a). Nta zindi mpinduka zijyanye n'umwanya zagaragaye imbere yimbere ya lamellar (Ishusho 6b). Ibinyuranye na byo, kugirango uhuze oxyde zitandukanye hamwe nibintu bitandukanye bya Fe2 + na Fe3 + muri SDSS ikonje ikonje, hashobora kugaragara imiterere idahwitse ya pseudopotential (Ishusho 6c, d). Fe3 + oxyde na / cyangwa (oxy) hydroxide nibintu byingenzi bigize ruswa yibyuma kandi byinjira muri ogisijeni namazi50. Kuri iki kibazo, birashobora kugaragara ko ibirwa bikungahaye kuri Fe3 + bikwirakwizwa mugace kandi bishobora gufatwa nkibice byangirika. Muri iki kibazo, icyiciro kiri murwego rushoboka, aho kuba agaciro ntarengwa k’ubushobozi, gishobora gufatwa nkikimenyetso cyerekana aho uturere twangirika dukora 51. Uku gukwirakwiza kudasanzwe kwa Fe2 + na Fe3 + hejuru yubukonje bwa SDSS bukonje burashobora guhindura imiterere yimiti yaho kandi bigatanga ubuso bunoze bwubuso bwa firime ya okiside yamenetse hamwe na ruswa ishobora kwangirika, bityo bigatuma materique yicyuma ikomeza kwangirika, bikaviramo kutagira imbere. no kugabanya ibiranga kurinda biranga passivating layer.
K. a, d K-bisobanura umugambi wuzuye hejuru yishusho ya X-PEEM. Ikigereranyo cya pseudoelectrode ishobora kuba (epseudo) ivugwa hamwe na K-bisobanura ibishushanyo mbonera. Umucyo w'ishusho ya X-PEEM nk'ibara ku gishushanyo cya 2 iragereranya neza na X-ray yo gukomera.
Ugereranije Cr ariko imiterere itandukanye ya Fe iganisha ku nkomoko itandukanye ya firime ya okiside yamenetse hamwe no kwangirika muri Ce-2507. Uyu mutungo wubukonje Ce-2507 irazwi. Kubijyanye no gushiraho okiside na hydroxide ya Fe mu kirere cyo mu kirere, ibisubizo bikurikira byafunzwe muri iki gikorwa nkibisubizo bitabogamye:
Ukurikije gupima X-PEEM, reaction yavuzwe haruguru yabaye mubihe bikurikira. Igitugu gito gihuye na Fe0 gifitanye isano nicyuma cyuma. Imyitwarire ya Metallic Fe hamwe nibidukikije biganisha ku gushiraho Fe (OH) 2 (kugereranya (5)), byongerera ibimenyetso Fe2 + muri XAS ya L edge ya Fe. Kumara igihe kinini mu kirere bizavamo gukora Fe3O4 na / cyangwa Fe2O3 oxyde nyuma ya Fe (OH) 252,53. Ubwoko bubiri bwa Fe, Fe3O4 na Fe2O3, burashobora kandi gukora muburyo bukingira Cr3 +, aho Fe3O4 ikunda imiterere imwe kandi ifatanye. Kubaho kw ibisubizo byombi bivanze na okiside ivanze (XAS-1 specran). Ikirangantego cya XAS-2 gihuye cyane na Fe3O4. Mugihe XAS-3 yerekanwe ahantu henshi yerekanaga ihinduka ryuzuye kuri γ-Fe2O3. Kubera ko X-imirasire idafunze ifite ubujyakuzimu bwa metero 50 nm, ibimenyetso biva murwego rwibanze bivamo ubukana bwinshi bwimpinga.
Ikirangantego cya XRD cyerekana ko igice cya Fe muri firime ya oxyde gifite imiterere itandukanye, ihujwe na Cr oxide layer. Bitandukanye na passivation iranga ruswa bitewe na inomomogeneité ya Cr2O317 yaho, nubwo urwego rumwe rwa Cr2O3 muri ubu bushakashatsi, byagaragaye ko kurwanya ruswa byaragaragaye muri uru rubanza, cyane cyane kuburugero rwakonje. Imyitwarire yagaragaye irashobora kumvikana nkuburinganire bwimiterere ya okiside yimiti yo murwego rwo hejuru (Fe) igira ingaruka kumikorere ya ruswa. Ihererekanyabubasha ryicyuma cyangwa ogisijeni ion muri lattice kubera stoichiometrie imwe yo hejuru (Fe oxide) no murwego rwo hasi (Cr oxide) 52,53 biganisha kumikoranire myiza (adhesion) hagati yabo. Ibi na byo, bitezimbere kurwanya ruswa. Kubwibyo, stoichiometry ikomeza, ni ukuvuga okiside imwe ya Fe, ni byiza guhita uhindura stoichiometric. Ubushyuhe bwa SDSS bufite ubuso bumwe kandi burinda urwego rwinshi, rutanga ruswa nziza. Nyamara, kuri SDSS ikonje ikonje, kuba hari ibirwa bya Fe3 + -bikungahaye munsi yuburinzi byangiza ubusugire bwubuso kandi bigatera kwangirika kwa galvanike ya substrate yegeranye, bigatuma kugabanuka kwa Rp (Imbonerahamwe 1) muri ecran ya EIS no kwangirika kwayo. kurwanywa. Kubwibyo, ibirwa byakwirakwijwe mubutaka bikungahaye kuri Fe3 + kubera guhindagurika kwa plastike bigira uruhare runini mubikorwa byo kurwanya ruswa, bikaba ari intambwe muriyi mirimo. Kubwibyo, ubu bushakashatsi bwerekana spekromicrografi yo kugabanya kugabanuka kwangirika kwangirika bitewe no guhindura plastike ya SDSS yize.
Ikigeretse kuri ibyo, mugihe isi idasanzwe ivanze mubyuma bibiri ikora neza, imikoranire yiki kintu cyongewe hamwe na materique yicyuma kugiti cye mubijyanye nimyitwarire ya ruswa ikomeza kuba ingorabahizi ishingiye kuri microscopi ya microscopi. Ikimenyetso cya Ce (kuruhande rwa XAS M-edge) kigaragara kumwanya muto mugihe cyo gukonja gukonje, ariko kikabura mugihe cyo guhindura ubushyuhe bwa SDSS, byerekana ko Ce yashyizwe muri materique yicyuma aho guhuza ibitsina. Nubwo imiterere yubukanishi bwa SDSS idatezimbere6,7, kuba REE igabanya ubunini bwibisobanuro kandi bikekwa guhagarika guhagarika imyanda ku nkomoko 54.
Mu gusoza, iki gikorwa kigaragaza ingaruka zuburinganire bwubutaka kuri ruswa ya 2507 SDSS yahinduwe na cerium mukugereranya ibigize imiti yibigize nanoscale. Twashubije ikibazo cyimpamvu icyuma kitagira ingese cyangirika kabone niyo cyaba gishyizwe hamwe na oxyde ikingira twiga twiga microstructure, imiterere yimiterere yimiterere yubutaka hamwe no gutunganya ibimenyetso dukoresheje K-bisobanura guhuriza hamwe. Bimaze kugaragara ko ibirwa bya Fe3 +-bikungahaye, harimo na octahedral hamwe na tetrahedral ihuza ibice byose bivanze na Fe2 + / Fe3 +, ni isoko yo gusenya firime ya okiside kandi ni isoko yo kwangirika kwa SDSS ikonje. Nanoisland yiganjemo Fe3 + iganisha ku kurwanya ruswa nabi kabone niyo haba hari stoichiometric Cr2O3 ihagije. Usibye iterambere ryakozwe muburyo bwo kumenya ingaruka ziterwa na nanoscale ya chimique itandukanye ya ruswa, iki gikorwa giteganijwe gutera imbaraga mubikorwa byubwubatsi kugirango tunoze kwangirika kwangirika kwibyuma bitagira umwanda mugihe cyo gukora ibyuma.
Gutegura ingobyi ya Ce-2507 SDSS yakoreshejwe muri ubu bushakashatsi, ibice bivanze, harimo na Fe-Ce master alloy bifunze hamwe nigituba cyiza cya fer, byashongeshejwe mu itanura ry’ibiro 150 byinjira mu ziko kugira ngo bitange ibyuma bishongeshejwe hanyuma bisukwa mu bishishwa. Ibipimo byimiti byapimwe (wt%) byashyizwe kumurongo winyongera 2. Ingot yabanje gushyuha mubice. Hanyuma ibyuma byashyizwe kuri 1050 ° C muminota 60 kugirango bikemuke, hanyuma bizimya mumazi kugeza ubushyuhe bwicyumba. Ingero zize zakozweho ubushakashatsi burambuye ukoresheje TEM na DOE kugirango bige ibyiciro, ingano yintete na morphologie. Ibisobanuro birambuye kubyerekeye ingero nibikorwa byakozwe murashobora kubisanga mubindi bisobanuro6,7.
Gutunganya icyitegererezo cya silindrike (φ10 mm × 15 mm) kugirango ukande ushyushye hamwe na axe ya silinderi ugereranije nicyerekezo cyo guhindura umurongo. Ubushyuhe bwo hejuru bwakorewe ku gipimo gihoraho kiri hagati ya 0.01-10 s-1 ku bushyuhe butandukanye buri hagati ya 1000-1150 ° C ukoresheje simulator ya Gleeble-3800. Mbere yo guhindura ibintu, ingero zashyutswe ku bushyuhe bwatoranijwe ku gipimo cya 10 ° C s-1 mu minota 2 kugirango ikureho ubushyuhe. Nyuma yo kugera ku bushyuhe bwubushyuhe, ingero zahinduwe ku giciro nyacyo cya 0.7. Nyuma yo guhindura ibintu, ihita izimya amazi kugirango ibungabunge imiterere. Noneho ingero zinangiye zaciwe ugereranije nicyerekezo cyo kwikuramo. Kuri ubu bushakashatsi bwihariye, twahisemo icyitegererezo cyahinduwe kuri 1050 ° C, 10 s-1 kubera microhardness yagaragaye cyane kuruta izindi ngero7.
Ingero nyinshi (80 × 10 × 17 mm3) z'icyitegererezo cya Ce-2507 zageragejwe ku byiciro bitatu bya asinchronous mashini ebyiri zo guhindura imashini LG-300, zitanga ibikoresho byiza bya tekinike mubindi byiciro byose byo guhindura ibintu6. Igipimo cyingutu no kugabanya umubyimba byari 0.2 m · s-1 na 5% kuri buri nzira.
Autolab PGSTAT128N yumuriro wamashanyarazi yakoreshejwe mugupima amashanyarazi SDSS nyuma yo gukonja kugera kuri 90% kugabanya umubyimba (1.0 ihwanye nukuri kwukuri) no gukanda kuri 0.7 kumurongo kuri 1050 oC na 10 s-1. Ikibanza gikoreramo gifite selile-electrode eshatu hamwe na electrode yuzuye ya calomel nka electrode yerekana, electrode ya grafite, hamwe nicyitegererezo cya SDSS nka electrode ikora. Ingero zaciwe muri silindiri zifite umurambararo wa mm 11.3, ku mpande z'umugozi w’umuringa. Noneho icyitegererezo cyasutswe hamwe na epoxy resin, hasigara ahantu hafunguye hafite cm 1 nka electrode ikora (hejuru yubushakashatsi bwa silindrike). Koresha ubwitonzi mugihe cyo gukiza epoxy no mugihe cyumusenyi hanyuma ugasiga kugirango wirinde gucika. Ubuso bukora burazengurutswe kandi busizwe hamwe na diyama isize ihagaritse ifite ubunini bwa micron 1, isukurwa namazi yatoboye na Ethanol hanyuma yumishwa mukirere gikonje. Mbere yo gupima amashanyarazi, ingero zasizwe zimaze iminsi zitagaragara mu kirere kugirango zikore firime isanzwe. Umuti wamazi wa FeCl3 (6.0 wt.%), Uhagaze hamwe na HCl kugeza pH = 1.0 ± 0.01, wakoreshejwe mukwihutisha kwangirika kwicyuma kitagira umwanda55, kubera ko kiboneka mubidukikije aho ioni ya chloride iba ifite imbaraga zikomeye za okiside na pH nke nkuko byagaragajwe na ASTM. Ibipimo bisabwa ni G48 na A923. Ingero zashizwe mubisubizo byikizamini mugihe cyisaha 1 mbere yuko hapimwa ibipimo kugirango bigere kuri leta yegereye guhagarara. Kubisubizo bihamye, ingero zishyushye kandi zikonje, urugero rwo gupima impedance intera yari 1 × 105 ~ 0.1 Hz, naho ubushobozi bwumuzunguruko (OPS) bwari mV 5, bwari 0.39, 0.33, na 0.25 VSCE. Buri kizamini cyamashanyarazi yicyitegererezo icyo aricyo cyose cyasubiwemo byibuze inshuro eshatu mubihe bimwe kugirango amakuru yororoke.
Kubipimo bya HE-SXRD, 1 × 1 × 1.5 mm3 ibyuma byurukiramende bya duplex byapimwe kumurongo wimbaraga za Brockhouse zifite ingufu nyinshi kuri CLS, muri Kanada kugirango ugereranye icyiciro 56. Ikusanyamakuru ryakorewe ku bushyuhe bwicyumba muri Debye-Scherrer geometrie cyangwa transport geometrie. Uburebure bwa X-imirasire ya kalibrasi ya LaB6 ni 0.212561 Å, ihwanye na keV 58, ikaba isumba cyane iya Cu Kα (8 keV) isanzwe ikoreshwa nka laboratoire ya X-ray. Icyitegererezo gishyirwa ku ntera ya mm 740 uvuye kuri detector. Ingano yo gutahura ya buri sample ni 0.2 × 0.3 × 1.5 mm3, igenwa nubunini bwibiti hamwe nubunini bwikitegererezo. Buri kimwe muri aya makuru cyakusanyirijwe hamwe hifashishijwe icyuma cya Perkin Elmer, icyuma gipima X-ray, pigiseli 200 µm, 40 × 40 cm2, ukoresheje igihe cyo kwerekana amasegonda 0.3 na frame 120.
Ibipimo bya X-PEEM bya sisitemu ebyiri z'icyitegererezo zatoranijwe byakorewe kuri sitasiyo ya nyuma ya PEEM y'umurongo wa Beamline MAXPEEM muri laboratoire ya MAX IV (Lund, Suwede). Ingero zateguwe muburyo bumwe bwo gupima amashanyarazi. Ingero zateguwe zabitswe mu kirere iminsi myinshi hanyuma zimanikwa mu cyumba cya ultrahigh vacuum mbere yo gushyirwaho na fotone ya synchrotron. Ingufu zumuriro wibiti ziboneka mugupima ion isohoka ya spekure kuva N 1 s kugeza 1 \ (\ pi _g ^ \ ast \) yakarere gashimishije hamwe na hv = 401 eV muri N2 hamwe ningufu za fotone kuri E3 / 2.57. Ikirangantego gikwiye cyatanze ΔE (umurongo ugaragara) ~ 0.3 eV hejuru yingufu zapimwe. Kubwibyo rero, ingufu za beamline zagereranijwe kuba E / ∆E = 700 eV / 0.3 eV> 2000 na flux ≈1012 ph / s ukoresheje monochromator ya SX-700 yahinduwe hamwe na Si 1200-umurongo wa mm - 1 ushushanya kuri Fe 2p L2,3, Cr 2p L2,3, Ni 2p L2,3, na Ce M4,5. Kubwibyo rero, ingufu za beamline zagereranijwe ko ari E / ∆E = 700 eV / 0.3 eV> 2000 na flux ≈1012 ph / s ukoresheje monochromator ya SX-700 yahinduwe na Si 1200-umurongo wa mm - 1 ufata Fe 2p L2.3, Cr 2p L2.3, Ni 2p L2.3, na Ce M4.5. Таким кромка Cr 2p L2,3, кромка Ni 2p L2,3 и кромка Ce M4,5. Niyo mpamvu, ingufu z'umuyoboro wa beam zagereranijwe nka E / ∆E = 700 eV / 0.3 eV> 2000 na flux ≈1012 f / s ukoresheje monochromator ya SX-700 yahinduwe hamwe na Si grating y'imirongo 1200 / mm kuri Fe edge 2p L2, 3, Cr edge 2p L2.3, Ni edge 2p L2.3, na Ce edge M4.5.因此，光束线能量分辨率估计为 E / ΔE = 700 eV / 0.3 eV> 2000 和通量≈1012 ph / s 通过使用改进的 SX-700 单色器和 Si 1200 线 mm - 1 光栅用于 Fe 2p L2,3 边缘、 Cr 2p L2,3 边缘、 Ni 2p L2,3 边缘和 Ce M4,5 边缘。因此 ， 光束线 能量 分辨率 为 为 为 δe = 700 EV / 0.3 EV> 2000 和 ≈1012 PH / S 通过 改进 的 SX-700 单色器 和 SI 1200 线 mm-1 光栅 于 Fe 2P 2P 2P L2.3 边缘、 Cr 2p L2.3 边缘、 Ni 2p L2.3 边缘和 Ce M4.5Rero, mugihe ukoresheje SX-700 yahinduwe monochromator hamwe na 1200 umurongo wa Si. 3, Cr edge 2p L2.3, Ni edge 2p L2.3 na Ce edge M4.5.Kwagura ingufu za fotone muri 0.2 eV intambwe. Kuri buri mbaraga, amashusho ya PEEM yafashwe amajwi akoresheje disiketi ya TVIPS F-216 CMOS ifite 2 x 2 binning fibre optique ihuza 1024 × 1024 pigiseli mumwanya wa 20 µm. Igihe cyo kwerekana amashusho ni amasegonda 0.2, ugereranije amakadiri 16. Ingufu zamashusho yifoto yatoranijwe muburyo bwo gutanga ibimenyetso bya kabiri bya elegitoroniki. Ibipimo byose bikozwe mugihe gisanzwe cyumurongo wa fotone ya polarize. Kubindi bisobanuro kubipimo, reba ubushakashatsi bwibanze 58. Nyuma yo kwiga umusaruro wa electron yose (TEY) 59 uburyo bwo gutahura no kuyikoresha muri X-PEEM, ubujyakuzimu bwubu buryo bugereranijwe kuri ~ 4-5 nm kubimenyetso bya Cr na ~ 6 nm kubimenyetso bya Fe. Ubujyakuzimu bwa Cr bwegereye cyane uburebure bwa firime ya oxyde (~ 4 nm) 60,61 mugihe ubujyakuzimu bwa Fe ari bunini kuruta ubunini bwa firime ya oxyde. XAS yakusanyirijwe hafi ya Fe L ni uruvange rwa oxyde oxyde XAS na FeO kuva matrix. Mugihe cyambere, ubukana bwa electron zasohotse biterwa nubwoko bwose bushoboka bwa electron zitanga TEY. Nyamara, ikimenyetso cyicyuma gisaba imbaraga za kinetic nyinshi kugirango electron zinyure murwego rwa oxyde, zigere hejuru, kandi zegeranijwe nuwasesenguye. Muri iki gihe, ibimenyetso bya Fe0 biterwa ahanini na electroni ya LVV Auger na electroni ya kabiri yoherejwe nabo. Byongeye kandi, ubukana bwa TEY bwatanzwe na electroni zangirika mugihe cyo guhunga electron 49 inzira irusheho kugabanya umukono wa spécral ya Fe0 mukarita yicyuma XAS.
Kwinjiza ubucukuzi bwamakuru muri cubes (X-PEEM data) nintambwe yingenzi mugukuramo amakuru afatika (imiterere yimiti cyangwa yumubiri) muburyo butandukanye. K-bisobanura guhuriza hamwe bikoreshwa cyane mubice byinshi, harimo iyerekwa ryimashini, gutunganya amashusho, kumenyekanisha imiterere idakurikiranwa, ubwenge bwubukorikori, hamwe nisesengura ryihariye24. Kurugero, K-bisobanura guhuza gukoreshwa neza muguhuza hyperspectral ishusho yamakuru62. Ihame, kubintu byinshi bifatika, K-bisobanura algorithm irashobora kubateranya byoroshye ukurikije amakuru yerekeye ibiranga (ibiranga ingufu za fotone). K-bisobanura guhuriza hamwe ni algorithm itera igabanywa ryamakuru mu matsinda ya K adahuzagurika (cluster), aho buri pigiseli iba ihuriro ryihariye bitewe nogukwirakwiza umwanya wa inomomogeneitike yimiti mubyuma bya microstructural. K-bisobanura algorithm igizwe nintambwe ebyiri: intambwe yambere ibara K centroide, naho intambwe ya kabiri igenera buri ngingo kuri cluster hamwe na centroide ituranye. Hagati yububasha bwa cluster isobanurwa nkibisobanuro byerekana imibare yamakuru (XAS spectra) yiyo cluster. Hariho intera zitandukanye zo gusobanura centroide ituranye nkintera ya Euclidea. Kubyinjiza ishusho ya px, y (x na y nibisubizo muri pigiseli), CK ni centre yububasha bwa cluster; iyi shusho irashobora noneho kugabanywa (ikusanyirijwe) mumatsinda ya K ukoresheje K-uburyo63. Intambwe zanyuma za K-bisobanura guhuza algorithm ni:
Intambwe 2. Kubara urwego rwabanyamuryango ba pigiseli zose ukurikije centroid iriho. Kurugero, ibarwa uhereye kuri Euclidean intera d hagati yikigo na buri pigiseli:
Intambwe ya 3 Shyira buri pigiseli kuri centroid ikwegereye. Noneho ubaze imyanya ya K centroid kuburyo bukurikira:
Intambwe 4. Subiramo inzira (ibigereranyo (7) na (8)) kugeza centroide ihuye. Ibisubizo byanyuma bya cluster ibisubizo bifitanye isano cyane nuburyo bwiza bwo guhitamo centroids63. Kuri PEEM yamakuru yububiko bwamashusho yibyuma, mubisanzwe X (x × y × λ) ni cube yamakuru ya array array ya 3D, mugihe x na y amashoka yerekana amakuru ajyanye (pigiseli ya pigiseli) naho λ axis ihuye nuburyo bwo kwerekana ingufu za fotone. K-bisobanura algorithm yakoreshejwe mugushakisha uturere dushishikajwe namakuru ya X-PEEM mugutandukanya pigiseli (cluster cyangwa sub-blok) ukurikije imiterere yabyo no gukuramo centroid nziza (XAS spectral curve) kuri buri analyte (cluster). Byakoreshejwe mukwiga ikwirakwizwa ryahantu, impinduka zaho zigaragara, imyitwarire ya okiside hamwe nimiterere yimiti. Kurugero, K-bisobanura guhuza algorithm yakoreshejwe kuri Fe L-edge na Cr L-edge mukarere gashyushye kandi gakonje X-PEEM. Imibare itandukanye ya K-cluster (uturere twa microstructural) yageragejwe kugirango ibone cluster nziza na centroide. Iyo igishushanyo cyerekanwe, pigiseli zoherejwe muburyo bukwiye bwa cluster centroids. Buri bara ryamabara rihuye hagati ya cluster, yerekana gahunda yimiterere yimiti cyangwa ibintu bifatika. Centroide yakuweho ni umurongo uhuza ibintu byiza.
Amakuru ashyigikira ibisubizo byubu bushakashatsi araboneka kubanditsi ba WC babisabwe neza.
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